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目的:优化并建立复方氨氯地平缬沙坦氢氯噻嗪片剂溶出度的测定方法,同时检测氨氯地平、缬沙坦和氢氯噻嗪3个组分的溶出度。方法:采用Zorbax SB-C18(3.0 mm×150 mm,5μm)色谱柱,以0.1%三乙胺(p H 2.8)-甲醇-乙腈为流动相进行梯度洗脱,流速0.8 m L·min-1,检测波长230 nm。结果:本方法系统适用性佳,3个组分分离度良好,空白辅料及强制降解产物不干扰3个组分的测定;氨氯地平、缬沙坦和氢氯噻嗪的线性范围分别为2.8~17.3μg·m L-1(r2=0.999 9)、32.0~200.2μg·m L-1(r2=0.999 4)和2.5~15.6μg·m L-1(r2=0.999 6);平均回收率(n=9)分别为100.6%(RSD=1.1%)、100.8%(RSD=0.62%)和101.0%(RSD=0.70%);定量限分别为0.33、0.13和0.12μg·m L-1;检测限分别为0.10、0.03和0.03μg·m L-1;供试品溶液在72 h内稳定;耐用性良好;该方法测得氨氯地平、缬沙坦和氢氯噻嗪在30 min溶出度分别为标示量的92%、94%和91%。结论:该方法适用于复方氨氯地平缬沙坦氢氯噻嗪片剂溶出度的检测。
OBJECTIVE: To optimize and determine the dissolution of compound amlodipine valsartan hydrochlorothiazide tablets, and to determine the dissolution of amlodipine, valsartan and hydrochlorothiazide. Methods: The gradient elution was carried out on a Zorbax SB-C18 (3.0 mm × 150 mm, 5 μm) column with 0.1% triethylamine (p H 2.8) -methane-acetonitrile as mobile phase at a flow rate of 0.8 m L · min -1 , Detection wavelength 230 nm. Results: The method has good system applicability, good separation of three components, blank adjuvant and forced degradation products without interfering with the determination of three components. The linear range of amlodipine, valsartan and hydrochlorothiazide were 2.8-17.3 μg · M L -1 (r 2 = 0.999 9), 32.0 ~ 200.2 μg · m L -1 (r 2 = 0.999 4) and 2.5 ~ 15.6 μg · m L -1 (r 2 = 0.999 6) 9) were 100.6% (RSD = 1.1%), 100.8% (RSD = 0.62%) and 101.0% (RSD = 0.70%). The limits of quantification were 0.33, 0.13 and 0.12 μg · m L-1, 0.10, 0.03 and 0.03 μg · m L-1, respectively. The test solution was stable within 72 h and the durability was good. The determination of amlodipine, valsartan and hydrochlorothiazide at 30 min were labeled 92%, 94% and 91%. Conclusion: This method is suitable for the determination of dissolution of compound amlodipine valsartan hydrochlorothiazide tablets.